Treating liquid with gas



Jan. 20, 1959 s. B. THOMAS IREAIING LIQUID WITH GAS Filed April 1e, 195s VENT OAS l n 2l 2O LEO. f

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8 PREHEATER o 0 o 3f 35?'2 9 35 |NVENTOR SAMUEL a. THOMAS H|s ATTORNEY 2,869,844 IC? A Patented Jan. 2o, v1.95.9

2,869,844 TRETnIoLIQUib lwlrnt GAS Samuel B. Thomas, Long Beach, Calif.,"assgnor-to Shell Development Company, New York, N. Y., a corporation of Delaware Application April i6, l11956, serial N. 578,256 s claims. (Ci. 'tzer-21) The present invention relates tok an improved method and apparatus for treating a liquid with a gas byfconcurrent ow wherein no internal power-driven elements, are used. The method and apparatus are of general applications, one specific process krbeing treatment of waste aqueous solution containing sulfur, such fas ammonium sulde, with air at elevated temperature-and pressureV to convert the sullideprimarily to thiosulphateprior to disposal of the aqueous solution; this treatment is described in the joint patent application of the inventor herein and Samuel York, tiled in the United States on March 23, 1955, Serial No. 496,314. A furtheriexample of fa process to which invention'can be applied is :the regeneration, by means of oxygen-containing gas, such as air, ofspent solutions (such as soda, Solutizer"slutiorfor "-Do'ctor solution) used to remove undesirable sulphur vcompounds from hydrocarbon oils. l o

In processes wherein a gas 'is 'dispersed within 'a liquid to 'effect intimate contact several problems are often encountered, namely, the sbdivis'ion ofthe gas intofsiifli ciently small bubbles to attain a large surface, the tribution of the bubbles to insure Contact with all'parts of the liquid, and the maintenanceof the dispersiohufqlf a sufficient time to permit the treatment to betornpletedl despite the tendency of the ascending bubbles to coalesce to form larger globules having a detrimentally reduced total surface. y, n f i# When a prolonged contacttime is requiredthe gas is sometimes dispersed at the bottom of a talla column, through whichy the liquid may also liovv vertically, extend the time required 'for ythe ascendingbubbles to rise to the liquid surface. Unfortunately fthe small bub-l bles or froth coalesce in rising through acolumn which is empty save for the gas and liquid and the subsequent contact between these fluids is poor. Moreoverpnatural circulation of the liquid in such-an empty columnzproduces channeling or short circuiting; This action leads to unequal residence times for variousl portions fotoni-the, liquid, and untreated or ineffectively treated liquid reaches the liquid outlet. t l y Liquid circulation within the column can be restricted to some extent by installing packing, battles, grids, 'or :the like. However, it has been observed that such expedients do not produce as effective a dispersion of the gas is desirable and, in fact, often act to coalesce thevgas bubbles into larger globules.

The foregoing ldiiiiculties can -be overcome lby using av series of treaters through which the 'gas and liquid'low concurrently. Such' installations have, however, hereto# fore provided for separate connections for the gas and liquid and have been costly to install. e

It is an object of this invention to provrdiei'an improved method and apparatus forefrectin'g con lnous', concurrrent contact between a liquid and a gas n "i the"ailtfc'fvl-` mentioned shortcomings ae overcome byy flowing the gas and liquid through a' series o'f separate vcontaSting `z`one's 2 or stages and redistributing the gas .and lliquid within each sage.' 1. .t

`Awfurther obj ect isl toiprovide'oanj improved apparatus for ^cariying out the method according to the foregoing Object Whhheas. ,fha-Steady .QW cf. bgth thefsas and liquid between stages j'injcontact with one' another ndterssniially Without 8111s ,1.19m 1 Further objects will be description. l In summary, according tothe invention the gas'fand apparent from the following v liquid are owedjconclurrently through a Vseries of separate, confined, pre`ferably superposed contacting zones within each of `which a :pool ofithe liquid is "maintained, byk admitting the gas andliquid continuously -into each zone as submerged` jets, Sand withdiawingth'e gas and liquid continuouslyffrom'ieachstage', in contact with one anotherby -guiding the gas 'collected at the top of each zone to Vmove witha lateral vandupwafrd kmotion toward the outflowing liquid stream and immediately commingling the gas with the 'outowing liquid. By operating inthis manner. the gas ispre'vented from :accumulating as large globulesfwhich are maintained Ain ipartbyjnterfacial tehsion. and which break at intervals to produce unsteady or ,slug ,type of l110W. The method oi v'ap'eratio'n lri'i'alels it possible 'to simplify the redistributions since both the liquid and gas are 'handled together. The rne'thod leiel'zts repeated redispersion of the gas 'within fthe liquid, therel by insuring the pr'es'enceot small bubbles throughout the treatment and affording the possibility of providing any desired contacting time Ibyilsingvk a suliicient 'number of contacting zones; the -liqui'djis rdispersed, Itherebyhbrealr; ing up those nnpanems that 'tene to' fcnanneuing; and the use of repeated submerged `gas vjeztsat 'the lowerpa'rts of the zones makes vpossible toemploy ernptyV cham;

bers, 'wherein the tendency of the 'gas bubbles to coalesce is minimized;

l Appa'ratiJs faccoidin'gvto. the linvention for,V carrying out the method includes series ,of chamberswhich,may be superpos'ed compartnjlentsy within a vertical1 column, each having near the bottom'thereof la distributing device .suitable for receiving aimi'xed flow of gasrvand liquid from a preceding (usually lower) stageof the series and for dispersin'g thek gas andzliquid ias', av plurality offsubmerge'd jets, Veach charinben(withl the ,possible exception of the lastp'in Ythe series.) having at `the top thereof an inclined roof whichgis advantageously conical .or dome-shaped has fa disf'cliarge opening for gas and liquid at an elevated and, preferably, `the `highest part thereof, said 'inlination `serving to deect gas .which is coalescedonrthe underside of the 4roof with a lateral ymotion to the said discharge opening and directly into the stream of liquid which vflows ,throughzthe opening, the said discharge opening being in communication with the inlet of ythe Vdistributor yof the nextvch'amber for theflow of both gas and liquid.` By this yconstruction the gas land liquid lflow smoothly from the top of the compartment in a mixed stream and alternating or slug flow, which wouldv occur were gas collectedrounder a` horizontal surface, is effecl tively avoided or minimized. The distributor isadvantageously of the type which has -a plurality o'f gas-'orifices and one or more openings through which normally only liquid-isdischarged but which can Aalso discharge gas when supplied =at rates greater' lthan the' capacity ofV the lgas orifices, Yto eiect smooth-flow 'o'f Vthe -gas and liquid and prevent dumpingfof` the gas through the 'first 'perforations encountered i The invention will be-further describ'ed with reference to the accompanying drawing forming a part of this 0 specification-and lshowing Vone preferred embodiment,

Figure 1 Yis a vertical sectional view of a contacting flow connections and auxiliary units used for the 'treat-A4 ment of sour water with air being shown diagrammatia11y;. Y i

Figure 2 is an enlarged detail view of a column of Figure l; and y p Figure 3 is a sectional view taken on the line 3*-3'of FigureZ. j A YReferring to- Figure 1, the contacting column 5 is provided with a plurality of dome-shaped'partitions 6 which divide the column into superposed compartments or chambers, each of which serves as a separate contacting portion-'of the zone. As used, for example, for the treatment of waste .sour water containing ammonium suliide with air at superatmospheric pressure, the water is admitted-'by a feed pump (not shown) at 7, preheated in a preheater 8, and commingled at 9 with air which is supplied under suitable pressure from a supply pipe 10 via a flow sensing element 11 and a flow'control valve 12 which may be operated automatically through a flow recording controller 13 in response to a signal through a control line 14. The commingled air and water enter the bottom of the lowermost compartment of the Icolumn via pipe 15 and a multi-jet distributor 16 (which is described hereinafter), ascend through the compartment with the gas bubbles ascending in relation to the water, and flow out through a discharge opening 17 at the highest part of the partition, which constitutes a sloping roof for the compartment. Both the gas and liquid ow through the discharge opening into a second and identically constructed distributor in the second compartment; the flow is the same in each compartment. The gas and liquid are withdrawn from the uppermost compartment, the top wall 18 of which is likewise dome-shaped and has a discharge opening 19 at the highest part, and ow through a pipe 20 and cooler 21 to a separating unit 22. This unit is shown diagrammatically to have a gas outlet pipe 23 at the top, by which the separated gas can be fed to a furnace, a Water drawoff pipe 24 at the bottom, by whichthe separated, treated water can be discharged at a rate determined by a flow control valve 25, and a liquid level controller 26 which senses the liquid level 27 within the tank and automatically actuates the valve through a control line 28.

The construction by which the smooth redistribution of gas and liquid is effected will now be described in detailwith references to Figures 2 and 3 of the drawing. Itgwill be noted that each distributor includes a distributorinlet29, which may take the form of an orifice, as shown, in a plate at the bottom of a feed or distributing chamber 30 and which is in communication with the discharge opening 17 at the highest part of the dome-shaped partition 6. The feed chamber may be secured to the partition by bolts 31 and has a plurality, e. g., eight, horizontal distributing pipes 32 which communicate at their inner ends with the feed chamber and which have gas-discharge perforations 33 on their upper surfaces, some perforations being directed upwardly and others having inclined axes. These perforations are preferably distributed as to number and/or varied as to size, e. g., made Ylarger toward the outer ends, to attain substantially uniform distribution of gas over the column cross section. The ends of the pipes 32 have openings which are larger than the perforations 33 and are preferably situated at a level some.- what below the pipe axis, although this'is notV in every case essential.v One mode of providing such depressed outlets is to thread elbows 34 at the pipe ends and fit nipples 35 thereto; rotation of the elbows permits the depths of open ends of the nipples to be adjusted. When the nipples do not extend vertically downwards it is desirable to arrange adjacent nipples in opposed relation, as shown in Figure 3, so as to oppose any whirling motion of the liquid such as would tend to coalesce the gas bubbles.

Because the distributing chambers 30 contain both gas and liquid and it is desired to distribute these fluids in l 4 like ratio among the several pipes 32, it is advantageous to have some turbulence within the distributing chamber.

A This can be insured by providing a suiciently high entrance velocity; when low or moderate liow rates are employed it is useful to constrict the orifice 29 as shown to induce such velocity and turbulence.

In operation, liquid fills each compartment and ascends slowly, while the gas bubbles rise more rapidly. Each compartment is otherwise empty and of limited height, so that the ascending gas bubbles are not greatly coalesced prior to impinging against the undersides of the inclined partitions 6 or the roof 18. They move laterally and upwards along this inclined surface toward the opening 17 or 19 and in doing so become coalesced; the coalesced gas then liowsdirectly and steadily into the said opening 17 or 19, together with liquid which is simultaneously liowing upward through the opening. By thus feeding the gas continuously from the side of the merging liquid current both gas and liquid are discharged steadily, substantially at the rates at which they are supplied to the distributor, and slug flow is substantially avoided.

Within the distributor pipes 32 a separation between gas and liquid occurs, although this may not be complete, and the ow is predominantly stratified. As a consequence mainly gas escapes upward through the perforations 33, which is dispersed as small bubbles throughout the liquid, while the liquid escapes from the terminal openings in nipples 35. By disposing these terminal openings at a level below the axes of the pipes 32 a slight liquid back-pressure is built up which can vary and becomes greater at increased gas flow rates; this tends to insure discharge of all the gas through all the perforations 33 over a range of flow rates and prevents excessive discharge of gas through the innermost perforations. When the gas flow rate exceeds the said range some gas flows out through the terminal openings, together with liquid. yThis feature limits the total pressure drop which can be developed in a distributor lby increased gas flow rates.

The column 5 is made tall enough to provide sutiicient contact time between the air and water to convert the sulfide in the water to thiosulfate. The air is maintained in a state of subdivision and intimate mixture thereof with all parts of the liquid is insured by leading the gas at the top of each compartment to the highest part thereof without the presence of any pocket wherein any gas glob ule can collect, and discharging it thence with steady flow into the next higher distributor, together with Water which is withdrawn from the top of the pool which fills the compartment to the top save for the gas moving along the underside of the partition. Gas is then injected as a multitude of submerged jets into the pool in the next higher compartment, and the water is also injected as a plurality of submerged jets. By thus repeatedly redistributing both the gas and the Water channelling is avoided. A particular feature of the invention is the discharge of the gas and liquid through a common outlet, asa mixed stream, while nevertheless substantially avoiding intermittent or slug flow of either of the uids. This greatly simplifies the construction, obViates the need for gasliquid separations at each stage, and makes the unit more compact.

The effectiveness of the construction is'illustrated by comparative tests performed intwo vertical contactors two inches in diameter and 20 inches high, one having no partitions between the top and the bottom and the other, illustrative of the invention, having a single 30 frustoconical partition with an opening at the top connected to a distributor in the form of a 1t-in. O. D. tube, l/2 inch long. Water containing sulfide was admitted at the rate of 200 cc. per min., at a pressure of 60 lbs. per sq. in. gauge together with air at a rate of 0.31 standard cu.

ft. per min. The contactor temperature was about 200V per million per pass, was determined after each pass and the sulfide oxidation rate was determined. lt was found that use of the partition and redistributor resulted in a 23% increase in the oxidation rate.

I claim as my invention:

l. Apparatus for the continuous treatment of a liquid with a gas concurrently within a series of contacting stages which comprises: a series of vertically superposed, enclosed contacting chambers 'each of which is adapted to be substantially filled with a separate pool of liquid and contains near the bottom thereof a distributor having a bottom inlet, said chambers being otherwise empty throughout the major parts of the heights thereof, each said chamber except the uppermost having a sloping roof which is situated wholly beneath the distributor of the next higher chamber and has at the highest part thereof an outlet opening extending over only a minor part of the chamber area and is continuously in upward communication with the inlet of the said higher distributor, said outlet openings being the only passageway interconnecting consecutive chambers of the series, each said distributor including con'rined duct means extending laterally from the said bottom inlet thereof and having a plurality of discharge openings situated higher than the said bottom inlet and distributed over the chamber area for the discharge of fluid as a plurality of submerged jets, means for supplying said gas and liquid continuously to the distributor inlet of the lowermost chamber, and means for discharging gas and liquid from the uppermost chamber.

2. Apparatus according to claim l wherein said distributing means includes a hollow body having an inlet through which the gas and liquid enter, said body having at least one terminal opening through which the liquid is discharged for the greater part and which is horizontally remote from said inlet and a plurality of outlet openings smaller than said terminal opening distributed between said inlet and the terminal opening through which primarily gas is discharged.

3. Apparatus for the continuous treatment of a liquid with a gas concurrently within aseries of contacting stages which comprises: a vertical column; a plurality of partitions within said column subdividing the column into compartments adapted to be substantially filled with said liquid, each said partitions sloping to a highest point at an inner part thereof; a distributor at the bottom of each compartment having an inlet through which said liquid and gas are supplied, a plurality of small gas discharge openings distributed over the column area, and larger terminal liquid discharge openings remote from the inlet and at alevel beneath that of said small openings, each said inlet of the distributor of each compartment above a partition being in communication with the highest part of the pocket defined beneath the said partition, means for supplying said gas and liquid continuously to the distributor inlet of the lowermost compartment; and means for discharging gas and liquid from the uppermost compartment.

References Cited in the le of this patent UNITED STATES PATENTS 363,173 schenck t May 17, 1887 1,209,490 Pindstoire Dec. 19, 1916 1,214,103 williams 1an. 30, 1917 1,436,886 Leibing Nov. 28, 1922 2,721,064 Reichardt oct. 1s, 1955 FOREIGN PATENTS 11,907 Great Britain Sept. 20, 1886 

